Dairy wax of increased flaking resistance



United States Patent 3,133,685 DAIRY WAX 0F INCREASED FLAKING RESISTANCE George A. Weisgerber, Cranford, and Arthur J. Reinsch,

Middletown, N.J., assignors to Esso Research and Engineering Company, a corporation of Delaware No Drawing. Filed June 1, 1961, Ser. No. 114,005

9 Claims. (Cl. 229-3.1)

The present invention is concerned with a new and improved wax composition and more particularly relates to the use of such a composition in the coating of paperboard milk cartons and the like. In accordance with the present invention, a superior dairy wax composition is formulated utilizing microwaxes secured from distillates in conjunction with a critical amount of white petroleum jelly. By utilizing the Waxes of this character, greater flexibility and better wax distribution is secured, thereby producing a high quality waxed container. The wax composition of the present invention is secured by utilizing a conventional refined parafiin wax in conjunction with critical quantities of particular microcrystalline waxes which have been produced from various distillates and a critical amount of a residual white petroleum jelly.

In the refining of hydrocarbon oils such as petroleum oils, it is known to segregate paraffin Waxes from so-called paraffin distillates, waxy lubes and the like. The overhead or paraffin distillate fraction for example has a boiling range of about 580 F. to 850 F. and a viscosity of about 80 S.U.S. at 100 F. A heavy lubricating oil distillate side stream, for example, has a boiling range of about 800 F. to 1000 F. and a viscosity of about 5070 S.U.S. at 210 F. The residuum comprises all the hydrocarbons boiling above this range and, for example, has a viscosity from about 150 to 200 S.U.S. at 210 F. Crystalline or paraffin Waxes produced from the paraffin distillates have melting points which range from about 120 F. to 150 F. This type of wax is characterized by large well-formed crystals that can be readily separated from the oil. Furthermore, this type of wax generally contains a relatively small amount of oil and can be refined with comparative ease.

The segregation of these waxes is secured by a number of processes. For example, it is known to chill the selected wax containing fraction in order to secure crystallization of the wax and to remove the wax crystals from the oil by filtering, centrifuging and the like. It is also known to use various dewaxing solvents such as liquid normally gaseous hydrocarbons, such as propane, as well as other solvents, such as methyl-ethyl ketone, methyl isobutyl ketone, and the like. 'It is also known to utilize in dewaxing operations solvent mixtures wherein one solvent comprises a wax precipitating solvent While the other comprises a solvent having a high solubility for oil. A solvent mixture of this character, for example, comprises 40% by volume of toluene and 60% by volume of methyl-ethyl ketone. In utilizing a mixture of this character, it has been the practice to add the mixture in toto or incrementally to the waxy distillate as it is being chilled. In dewaxing operations, it is also known to use various filter aids and other agents in order to render the dewaxing and filtering operations more efficient.

The wax segregated from the hydrocarbon oil, usually ter ed slack wax, contains from about 10% to 40% of oil. The slack wax is refined usually by conventional sweating to produce crude scale Wax in a manner to reduce the oil content to less than about 5% by weight. The slack wax may be distilled to obtain the desired boiling range wax prior to sweating, if desired. This crude scale wax generally has an oil content of about 2% to 3% by weight. In order to remove this oil from the scale wax to produce a refined wax, such as refined paraffin wax, having an oil content below about .5 usually below about 3%, various procedures have been proposed solvent deoiling process, to remove oil from the wax.

In this, the wax is dissolved in such solvents as methyl isobutyl ketone, methyl ethyl ketone, or mixtures of methyl ethyl ketone and toluene in a ratio of approximately 75 to 25, respectively. The wax solution is cooled to produce crystallization and the crystallized wax is removed by a process such as filtration. The filter cake of crystallized wax may be washed with cold solvent to remove occluded oil solution. The wax so produced may be an unfinished refined parafiin wax or an unfinished microcrystalline wax, depending on the nature of the slack wax feed and on the selection of crystallization conditions. After oil removal from the wax, it is subjected to a finishing process such as clay percolation or hydrofining. In the latter, the process involves treating the unfinished wax with hydrogen gas at a rate of about 0.5-1.0 volume of wax per hour, at 500-800 p.s.i., at 500-600 F., in contact with cobalt molybdate catalyst. Or, at lower pressures such as 200 p.s.i., a nickel catalyst may be used. The hydrogen treated wax product is greatly improved with respect to color, odor and purity.

It is also known in the art to segregate microcrystallin Waxes from residual oils. As pointed out heretofore, these waxes are normally produced from residuums which boil above about 1000 F. and have viscosities in the range from 150 to 200 S.U.S. at 210 F. These microcrystalline waxes are characterized by very minute crystalline forms and which melt in the range from about 145 F. to 190 F. These microcrystalline waxes from residual oils are of a relatively high melting point and of different crystalline structure. The microcrystalline waxes may be prepared from any of the paraffin or mixed base crude oils. The undistilled residue may be treated with sulfuric acid and neutralized to remove the tarry matter and unsaturated hydrocarbons. The undistilled residue also may be deasphalted. The treated stock, containing a fairly high percentage of wax as evidenced by a very high pour point, may be dewaxed by blending with a dewaxing solvent, such as propane, methyl. ethyl ketonebenzol, or petroleum naphtha and chilled, and filtered or centrifuged to separate the waxy fraction from the re: sidual lubricating oil solution.

This dewaxing operation produces a Wax fraction containing some oil and solvent. The wax afterremoval of the solvent has a melting point of from about to 180 F. The wax may be again put in solution with more solvent or naphtha and chilled and filtered or recentrifuged to further reduce the oil content. The wax which separates in either of these operations is referred to as crude microcrystalline wax. The Wax separated in the second crystallization process after stripping to remove solvent is fairly dry and of a low oil content. This wax should not be confused with petroleum jellies which contain large amounts of oil. The microcrystalline wax may be again put into solution with naphtha and filtered through clay or an equivalent material in order 10 111!- prove its color. The clay filtered solution is distilled to remove the naphtha, the residue being a refined microcrystalline wax having a melting point Within the range of about to F. Alternatively, the microcrystalline wax may be hydrogen treated to improve its color and odor, such as by hydrofining at about 600 F., 600 p.s.i. of hydrogen, using cobalt molybdate catalyst. The source of the crude oil and the oil content of the refined microcrystalline product will affect the melting point of the final wax product. The refined microcrystallin wax,

a sometimes called amorphous wax, is as pointed out of a very small crystal structure.

It is also known in the art to segregate microcrystalline waxes from distillate lubricating oils. These distillate type microcrystalline waxes differ in characteristics from the residual type microcrystalline waxes hereinbefore described. Thus, the distillate waxes are lower in viscosity and are generally finished to a higher degree of purity, such as freedom from color and odor. Furthermore, the distillate microcrystalline waxes have two advantages over the residual microcrystalline waxes from the standpoint of ease of manufacture. Namely, first, the distillable nature of the wax makes it possible to manufacture specific microcrystalline wax fractions for use in specific product applications; and, second, the distillate waxes can be more readily and more economically refined with respect to color and odor than can the residual microcrystalline waxes. These features of distillate microcrystalline wax (low viscosity, high purity, select fractionation, economy of finishing) have been found to be of particular value in the present invention.

The distillate microcrystalline waxes are manufactured from distilled waxy lubricating oil fractions from crude oil. These fractions will vary with regard to distillation range, depending upon the desired viscosity grade of the lubricating oil ultimately produced. Thus, a number of fractional cuts may be taken across the lubricating oil distillation range, to produce different lubes. The entire range may cover a distillation from about 650-1 180 F. (760 mm. basis). Each of the fractional waxy lubricating oil cuts is processed to remove the waxy components by a process such as dewaxing by solvent crystallization. As hereinbefore described, this comprises dissolving the waxy distill-ate in such solvents as methyl ethyl ketone, methyl isobutyl ketone and mixtures of methyl ethyl ketone and toluene, cooling the solution to cause crystallization of the wax, then filtering to separate the lubricating oil and the slack Wax. The slack wax is then processed to further remove oil from it by a procedure such as solvent deoil-ing. In this operation, the excess oil is removed from the slack wax, by the solvent crystallization technique, while at the same time the solvent and temperature conditions are controlled to achieve a fractional crystallization of the wax fraction. Thus, a slack wax may be crystallized first at a relatively high temperature, to separate the most crystalline, paraffinic and high melting wax components present in the slack wax as the solid phase. The melting point may range from 140 to 190 F., depending on the properties of the slack wax feed and the crystallization temperature. The filtrate phase is then further cooled to cause a second crystallization of wax which is microcrystalline in nature, and of lower melting point than the first wax cut. Waxes in this fraction vary from 125 to- 140 F. melting point. By selection of the solvent composition and crystallization temperature, the exact properties of the separated wax can be controlled. The filtrate from the second crystallization contains the oil which was removed from the wax fractions. Both the first and second fractions of wax contain about 0.2 to 1.5% oil, this generally being 0.3 to 1.0% oil. These deoiled wax fractions may then be finished to the desired degree of purity with respect to color and odor by one of several methods, such as the hydrogen treating (hydrofining) or adsorption (clay percolation) methods previously described. As a final manufacturing operation, the paraffin or microcrystalline wax may be distilled again, to further separate specific wax fractions.

In compositions of the current invention, it is particularly important that microcrystalline waxes of the distillate type rather than microcrystalline waxes of the residual type, be employed as components in the dairy wax coating formulations.

The hereinbefore mentioned residual microcrystalline wax or distillate microcrystalline wax may be characterized as being waxes of very small crystal structure having melting points within the range of 140 to 180 F. In contrast to these, the term petrolatum is used in this application to cover the residual type products of amorphous nature, having melting points in the range of about to F., and oil contents in the range of about 5 to 40%. Thus, petrolatums are characterized by relatively high oil contents with some medicinal grades (petroleum jelly such as Vaseline) being highly refined with respect to color, odor, and purity. The refined petrolatums are treated to give good color, odor, and purity properties, by very careful adsorption methods, such as clay percolation. In refining of petrolatum jelly, it is important that the gel structure, or unctuous nature of the product, be not destroyed by severe chemical treating. Thus, acid treating is not employed with petrolatum jelly.

It is also known in the art that the Wax formulations used for milk carton coating are among the most critical The 1 ance quality in one or two aspects, but which also have certain quality weaknesses. The overall quality for dairy waxes is controlled by a number of rigid tests. One test is the flaking test which measures the degree to which wax particles will flake ofl the carton and adulterate the milk. Other rigid tests for wax for milk coating car-tons are the bottom wax accumulation test, the bottom wax flowing test, the cold flexibility test, the consumption test, as well as the appearance of the coating, the dye coverage, and the rub-oil.

However, the most important factors are those that concern the very undesirable flaking, since the excessive wax floats in the milk and is of immediate deep concern to the users. Flaking is a prime cause of customer complaint. The Flaking Test procedures are as follows for waxed milk cartons after passing through the waxing machine and after filling with a liquid at 38 F., the normal filling temperature.

Method A.Five to ten filled test cartons are each dropped eight times from a height of 7 inches onto a rail frame, i.e. a group of A rods spaced apart, 4" long for /2 gallon cartons and 3" long for quart cartons. The displaced flakes are filtered out, washed, dried and weighed.

Method B.Same as Method A except that the cartons are dropped onto a metal plate slightly greater than the size of the carton bottom, having the corners of the plate turned up (dog-eared) to a height of Method C.Thirty-six filled test cartons are each dropped twice from a height of 5 inches onto the corner plate described in Method B for half gallons. For quarts, the 36 cartons are dropped 6 times from a height of 5 inches.

The Bottom Wax Accumulation Test is a visual rating of the relative amount of wax that has run down the sides of the carton and has gathered inside of the carton at the bottom. The accumulation is rated as light, moderate, or heavy. Greater accumulation tends to lead to more flaking.

The Bottom Wax Flowing Test determines the amount of molten or semi-molten wax that flows across the bottom of the carton due to the vigorous motion of the carton as it travels through the cooling or wax hardening section of the dairy machine. The molten lava-like flow doesinot re-fuse with the main body of wax, but tends to solidify separately from the main coating, in the form of a thin sliver or overlayer on the bottom, in the corners, or washed up the sides. This overlayer is very readily displaced if the carton receives a mechanical shock due to rough handling. Flowing is a phenomenon depending very much on the machine type, and on the routing of the carton within the cooling chamber. In some machines flowing does not occur and is not contributory to flaking. In other machines, where flowing can occur, it becomes an extremely serious problem. Flowing is evaluated by visual observation of the inside coating of the carton and the displaced flakes.

The Cold Flexibility Test determines cold flexibility rather than brittleness. Cold flexibility is desired in the wax coatings in order to resist mechanical shock. The cold flexibility is evaluated by cutting ofi the bottom of a test carton which has been filled with liquid at 38 F., and rapidly flexing the bottom through an angle of about 90 degrees. The rating of poor to very good is made on the basis of audible brittleness, the degree of cracking and the separation of ruptured flakes from the bent paperboard.

Consumption is the rate of wax usage per thousand cartons, measured by weighing cartons before and after waxing. High wax consumption generally tends to produce high wax accumulation and flowing and high flaking.

.Also, a reasonable amount of consumption must always be maintained in order to achieve a uniform protective covering of the paperboard.

In accordance with the present invention, a conventional refined paraflin wax is used in conjunction with critical amounts of distillate microcrystalline waxes and in conjunction with a critical amount of a residual petrolatum or white petroleum jelly or pharmaceutical petrolatum.

The white petroleum jelly or pharmaceutical petrolatum is a residual fraction of petroleum, obtained by deasphalting and heavy treating of residual lube petrolatums by adsorption methods using materials such as clay, bauxite, silica or the like in percolation or contacting equipment. The adsorption is carried out to a degree that the petrolatums are highly refined or purified. It is important that this petrolatum be substantially more refined in terms of color or aromatic content than are the amber residual microwaxes that have heretofore been commonly used in dairy waxes.

A conventional refined paraflin wax is used in conjunction with critical amounts of various microcrystalline wax produced from distillate sources and the petroleum jelly. These waxes of the present invention have outstanding and unusual advantages over other commercial dairy waxes. The waxes of the present invention avoid or minimize the bottom accumulation and flowing, and impart desirable cold flexibility, leading to an overall reduction in the level of the flaking. The wax of the present invention will also have better performance by reason of better cold flexibility characteristics.

Thus, a very important part of this invention is that these characteristics are achieved utilizing distillate microwaxes and a white petroleum jelly. Advantages are thereby realized with regard to purity, availability and cost. In cases where control of accumulation and flowing are desired or necessary, it is seen further that the congealing point of the preferred dairy wax shouldbe about 140 F. minimum, and preferably about 145 F.

The base wax formulations of the present invention are characterized by having the following constituents.

TABLE I 7 Percent by weight Constituents Range Preferred Refined paraffin wax (about 3% oil) -90 V 79 Microcrystalline A 8-12 10 Microcrystalline 13.-.. 3-12 5 Micrficrystalline C 37 5 Polyethylene (7000 molecular wt .12.0 .5 V V Polyethylene (12,000 molecular wt.) 1-2. 0 .5 Oxidation inhibitor 0003-. 001 0005 The refined paraflin wax is secured as described heretofore and comprises a deoiled slack wax to produce a refined wax having an oil content less than about .3% by weight.

The microcrystalline waxes are secured from distillate lube oil petrolatums' by recrystallization techniques utilizing a solvent comprising methyl ethyl ketone and methyl isobutyl ketone.

Microcrystalline wax A was secured by treating a distillate waxy lubricating oil stream of about SAE 30 with a solvent at a temperature of 20 F. with approximately 3 volumes of solvent to one volume of oil. Under these conditions, a slack wax was produced and separated from the lubricating oil. The slack was then redissolved in about 6 volumes of solvent to one volume of wax and cooled to 65 F. to achieve crystallization. Under these conditions, l55l60 F. melting point paraffin wax was removed. The filtrate was further cooled to a temperature of 51 F. with treatment of 8 volumes of solvents to one volume of wax, to crystallize microcrystalline wax A.

Microcrystalline wax B was secured by treating a waxy lubricating oil distillate of SAE 60 with 5 volumes of solvent to one volume of waxy lubricating oil distillate at a temperature of 25 F. Under these conditions, a slack wax was produced which was then redissolved with heat in about 6 volumes of solvent to one volume of wax plus oil feed and cooled to about 96 F. The wax fraction precipitated comprised crude microcrystalline wax B.

The filtrate was further cooled with 7 volumes of solvent to one volume of wax plus oil feed. At the temperature of 48 F., the crude microcrystalline wax C was collected.

The crude microcrystalline waxes were finished by hydrogen treating at 600 F. and 600 p.s.i., using cobalt molybdate catalyst, to improve their quality with respect to color, odor, and purity. The inspections of the respective wax fractions are listed in Table II.

TABLE II T ypzcal Wax Component Inspection:

Identity Microcrystalline A B C Description Second First erys- Second Refined crystallizatallization crystallizabase Wax tion from from tion from ketone MIBK MIBK (MIBK) deoiling of deoiling of deoiling of SAEv 60 SAEGO SAE 30 slack wax slack wax slack Wax Gougealing pt., F 182 136 128 Viscosity at 210 F., cs- 6. 5 11.0 11.4 3. 8 Distillation, F.:

Inspection of Petrolatum Snow White #2 Petrolatum M. pt., F Congealing pt., F Oil content, Layton percent (MEK at MEK soluble at 70 F., percent Distigagzion, vac. F., mm

than about 0.3% oil, of microcrystalline wax A, 5% of microcrystalline wax B, and 5% of microcrystalline wax C. The bas wax also contained .5 of polyethylene 7,000 molecular weight and 0.5% of polyethylene 12,000 molecular weight. To the base wax was added 1.6 to 5% of petrolatum which materially reduced the flaking of the wax, as illustrated in the following Table IV.

TABLE IV Dairy Wax Containing Petrolatum Improves Flaking Control Test arrangement:

Location D Machine S, gallon Wax temperature, 190 F.

WaxNo I II III IV V VI Composition +1.6% pet- +2%pet- +5% pet- Competi- Competitive rolatum. rolatmn. rolatum. tive comcommermercial cial wax.

wax.

Consumption, lbs./ 48.7. 49.5 49.9.. 51.8 48.9 55.3.

1000 n. Flaking, gin/1000 ctn:

MethodA 9 4 6-.- 1.4 9 22. MethodB 13 6 0.2 66 18. Cold flexibility Good Verygood..- Very good.-. Very good... Good Poor. Bottomwax Moderate..- Moderate-.- Moderate..- Moderate..- Heavy..- Heavy.

accumulation. Flowing No No No No Congealing pt., F-.. 145

aromatic content than are the amber residual microwaxes that have been commonly used in dairy waxes. With petrolatum the color content is very low, odor is negligible, and the material meets U.S.P. requirements.

The high quality of the wax composition of the present invention may be readily appreciated by the following examples wherein the various wax compositions were tested utilizing several field tests and full-scale machines.

Test location Machine model Criticality F, quart.-- Bottom wax accumulation.

Additional data were obtained in another machine, which is particularly critical with regard to the flaking tendency of the waxed cartons. Results are given in Table V. The base wax I of these tests is the same as the base wax I in the tests of Table IV. The wax I gave moderate flaking. Adding 2.4 to 7.1% of petrolatum gave immediate and substantial reduction in flaking. The improved performance is primarily due to the better cold flexibility imparted by the petrolatum. It is noted in Table V that the formulations I, II, III, and IV containing only 5% microcrystalline B do not provide complete control over bottom wax flowing. This is corrected by use of a slightly higher content (10%) of microcrystalline C, gallon Accumulation and flowing. V2 Accumulatwn- B, as in wax V. The resultlng flaking 1s practically ml /2 gram per thousand cartons.

TABLE V Dairy Wax Containing Petrolatum and High Melting Wax Gives Good F laking and Flowing Control Test arrangement: Location S Mach e C, gallon Wax No I II III IV V +71% pet- Composition +2.4% pet- +4.7% petrolatum +71% petrolatum rolatum rolatum +5% microerystalline B Waxing temp., F 19 19 19 18 185. Consumption, lbs./ 37.9 38.2 38.2 39.1 39.1.

1000 ctn. Flaking, gum/1000 ctn. 18- 3.2-- 1.1-. 6.4.- 0.5.

method Cold flexibility Good to v Very good... Very good... Very good... Very good--. V. good to good. excellent. Bottom Wax Light Light Light Lt. to Lt. to Light.

accumulation. moderate. moderate. Bottom Wax fiowing.. .---.do ..d0 .-d0 Moderate.-- Moderate.. Nil.

Various tests were conducted to determine the effect of the added petrolatum. The tests were carried out in a Model S full-scale daily machine and the eflect of the added petrolatum is clearly shown in the test data of Table IV. The base case is wax I which, in essence, comprises 79% of a refined paraflin wax containing less From the above it can be seen that the preferred wax composition is wax V. It contains the two microcrystalline waxes A and C which were prepared by deep deoiling to maximize the non-normal paraflin content. This is desirable to provide wax flexibility and toughness. Also, it contains the high melting microcrystalline B to control wax distribution and minimize wax flowing.

In accordance with the present invention, the base wax composition to which the petrolatum is added is a critical part of the current invention. The base wax should be a wide cut and must have a congealing point of over 125 F., preferably at or above 130 F. The base wax should also have added to it minor proportions of the high melting wax component such as microcrystalline B, so that the final dairy wax composition will have a congealing point of 135 F. minimum, preferably above 140 F.

While the wax compositions of the present invention were particularly developed and designed to serve as coatings for milk cartons, it will be appreciated that these wax compositions will also find useful application in other fields. Thus, paper or paperboard products coated with waxes of the current invention can be effectively used for packaging of orange juice, grape juice, cottage cheese, frozen food, and the like. In such applications, the excellent covering quality of the wax, its flexibility at low temperature, resistance to thermal or mechanical shock, good purity qualities and so forth, are of particular value. Similarly, the wax may be used as a direct coating of foodstuffs or other items, without paper, where the packaged material is to be subjected to conditions of low temperature, mechanical shock, and the like.

What is claimed is:

1. Improved wax coating composition which comprises essentially a refined paraffin wax present in the concentration from about 70 to 90% by weight, a first microcrystalline wax secured from a first distillate present in the concentration of from about 8 to 12% by weight, a second microcrystalline wax secured from a second distillate present in a concentration from about 3 to 12% by weight, a third microcrystalline wax secured from said second distillate present in a concentration of from about 3 to 7% by weight and about 0.5 to 10% by weight of a white petroleum jelly having an initial boiling point of about 246 F. and a 50% distillation at about 580 F. at 1 mm. vacuum, said first distillate comprising a waxy lube oil having an SAE viscosity of about 20 to 40 and said second distillate comprising a waxy lube oil having an SAE viscosity of about 55 to 65.

2. Composition as defined by claim 1 wherein said refined paraffin wax is present in a concentration of about 79% by weight, wherein said first microcrystalline wax is present in a concentration of about 10% by weight, wherein said second microcrystalline wax is present in a concentration of about by weight, wherein said third microcrystalline wax is present in a concentration of about 5% by weight, and wherein said petroleum jelly is present in a concentration in the range from about 1 to 5% by weight.

3. Composition as defined by claim 2 wherein said composition comprises about 1% of polyethylene.

4. Composition as defined by claim 3 wherein said polyethylene comprises about 0.5% by weight of a polyethylene of about 7,000 molecular weight and about 0.5 by weight of a polyethylene of about 12,000 molecular weight.

5. Composition as defined by claim 1 wherein said first microcrystalline wax is secured from a waxy lube oil distillate after initially solvent precipitating a wax having a melting point of 155160 F. and thereafter cooling the filtrate to produce said first microcrystalline wax.

6. Composition as defined by claim 5 wherein said wax having a melting point of -155-160 F. is removed at a temperature of about 65 F. and wherein said first microcrystalline wax is precipitated at a temperature of about 50 F.

7. Composition as defined by claim 1 wherein said second microcrystalline wax is produced from a waxy lube distillate by precipitating a slack wax therefrom and thereafter deoiling said slack wax to produce said second microcrystalline wax at a temperature of about to F thereafter separating a filtrate to a temperature in the nange from about 40 to 5 0 F. and precipitating said third microcrystalline wax.

8. An improved wax covered carton which comprises in combination a paper carton having adhered thereto a wax composition which comprises essentially a refined paraffin wax having a congealing point of about 128 F. present in a concentration from about 70 to 90% by weight, a first microcrystalline wax secured from a first distillate present in a concentration of from about 8 to 12% by weight and having a congealing point of about 130 F., a second microcrystalline wax secured from a second distillate present in a concentration from about 3 to 12% by weight and having a congealing point of about 182 F., a third microcrystalline wax secured from said second distillate present in a concentration of from about 3 to 7% by weight and having a congealing point of about 136 F. and an effective amount of a white petroleum jelly having an initial boiling point of about 246 F. and a 50% distillation at about 580 F. at 1 mm. vacuum, said first distillate comprising a waxy lube oil having an SAE viscosity of about 20 to 40 and said second distillate comprising a waxy lube oil having an SAE viscosity of about 55 to 65.

9. Improved wax coating composition which comprises essentially a refined parafiin wax having a congealing point of about 128 F. present in a concentration of from about 70 to 90% by weight, a petrolatum present in a concentration of from about 0.5 to 8% by weight, said petrolatum being secured as a residual fraction of petroleum having a congealing point of 114 F. and boiling ing the range from about 240 to 670 F. and having a 70% distillation point at 1 mm. pressure, a first microcrystalline wax secured from a lube distillate having a congealing point of about 130 -F. and boiling in the range from about 470 to 720 F. at 10 mm. pressure, a second microcrystalline wax secured from a second lubricating oil distillate present in a concentration of from about 3 to 12% by weight, said second microcrystalline wax having a congealing point of about 182 F. and boiling in the range from about 480 to 700 F. at 1 mm. pressure, a third microcrystalline wax secured from said second distillate present in a concentration from about 3 to 7% by weight, said third microcrystalline wax having a congealing point of about 136 -F. and boiling in the range from about 400 to 700 F. at 1 mm. pressure.

References Cited in the file of this patent UNITED STATES PATENTS 2,733,225 Smith Ian. 31, 1956 2,846,375 Annable et a1. Aug. 5, 1958 2,903,408 Moyer Sept. 8, 1959 2,967,817 Marple et al. Jan. 10, 1961 2,988,528 Tench et al June 13, 1961 FOREIGN PATENTS 597,090 Canada Apr. 26, 1960 

1. IMPROVED WAX COATING COMPOSITION WHICH COMPRISES ESSENTIALLY A REFINED PARAFFIN WAX PRESENT IN THE CONCENTRATION FROM ABOUT 70 TO 90% BY WEIGHT, A FIRST MICROCRYSTALLINE WAX SECURED FROM A FIRST DISTILLATE PRESENT IN THE CONCENTRATION OF FROM ABOUT 8 TO 12% BY WEIGHT, A SECOND MICROCRYSTALLINE WAX SECURED FROM A SECOND DISTILLATE PRESENT IN A CONCENTRATION FROM ABOUT 3 TO 12% BY WEIGHT, A THIRD MICROCRYSTALLINE WAX SECURED FROM SAID SECOND DISTILLATE PRESENT IN A CONCENTRATION OF FROM ABOUT 3 TO 7% BY WEIGHT AND ABOUT 0.5 TO 10% BY WEIGHT OF A WHITE PETROLEUM JELLY HAVING AN INITIAL BOILING POINT OF ABOUT 246* F. AND A 50% DISTILLATION AT ABOUT 580* F. AT 1 MM. VACUUM, SAID FIRST DISTILLATE COMPRISING A WAXY LUBE OIL HAVING AN SAE VISCOSITY OF ABOUT 20 TO 40 AND SAID SECOND DISTILLATE COMPRISING A WAXY LUBE OIL HAVING AN SAE VISCOSITY OF ABOUT 55 TO
 65. 